US4717551A - Titanium-based alloy used as a gettering material - Google Patents

Titanium-based alloy used as a gettering material Download PDF

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Publication number
US4717551A
US4717551A US06/751,972 US75197285A US4717551A US 4717551 A US4717551 A US 4717551A US 75197285 A US75197285 A US 75197285A US 4717551 A US4717551 A US 4717551A
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United States
Prior art keywords
sub
alloy
titanium
based alloy
hydrogen
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Expired - Lifetime
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US06/751,972
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English (en)
Inventor
Otto Bernauer
Klaus Ziegler
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Daimler Benz AG
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Daimler Benz AG
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Assigned to DAIMLER-BENZ AKTIENGESELSCHAFT reassignment DAIMLER-BENZ AKTIENGESELSCHAFT ASSIGNMENT OF ASSIGNORS INTEREST. Assignors: BERNAUER, OTTO, ZIEGLER, KLAUS
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Classifications

    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J7/00Details not provided for in the preceding groups and common to two or more basic types of discharge tubes or lamps
    • H01J7/14Means for obtaining or maintaining the desired pressure within the vessel
    • H01J7/18Means for absorbing or adsorbing gas, e.g. by gettering
    • H01J7/183Composition or manufacture of getters
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C27/00Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
    • C22C27/02Alloys based on vanadium, niobium, or tantalum

Definitions

  • Getter materials have been used for many years in industry and in the laboratory, for example for absorbing harmful residual gases from vacuum pipes, apparatus filled with noble gas, vacuum systems and the like. For these applications it is frequently necessary to activate the getter material at relatively low temperatures (ideally below 500° C.) in order to avoid harmful thermal effects on the housing walls.
  • the customarily used getter materials made of zirconium or zirconium-aluminium alloys require activation temperatures of 700°-900° C. and, in the most favorable case, of only partial activation, of about 500°-700° C.
  • getter material which has good soption properties and can be activated at very low temperatures.
  • the alloys are prepared in a manner known per se by melting together the alloy constituents or appropriately selected prealloys under protective gas, by first of all in a manner known per se preparing a melt from the higher-melting constituents and then adding the lower melting constituents, in order to minimize the rates of evaporation. To reduce the oxygen content of the alloy, the melt is then deoxidized in conventional manner by addition of known deoxidizing agents, lanthanum, misch metal and the like.
  • the solidified melt is then pulverized under protective gas.
  • the alloy is capable of absorbing large amounts of hydrogen at about room temperature and of rereleasing the amounts at temperatures of about 100°-150° C. This absorption-desorption process leads to a comminution of the alloy particles, so that by repeatedly loading and unloading the alloy with hydrogen the particle size of the alloy can be reduced to less than 1 um.
  • the resulting large surface area combined with short diffusion paths is responsible for a particularly powerful absorption effect per gram of the getter material.
  • the getter material can likewise be activated by loading and unloading the alloy with hydrogen, for example by introducing the hydrogen-loaded getter material into the operating space and then removing the hydrogen by pumping at moderate temperatures between room temperature and about 150° C., exceptionally however at even higher temperatures.
  • the getter material thus activated has an excellent absorption capacity for nitrogen, water, oxygen, carbon oxides, hydrogen and the like.
  • it is also possible to use the hydrogen-loaded getter material for example if the release of small amounts of hydrogen is not critical or the operating atmosphere is H 2 , since the absorption capacity for the other gases is barely affected by the hydrogen content, if at all.
  • Alloys which have been found to be particularly suitable are alloys of the formula TiV 1 .8 Fe 0 .2, TiV 1 .6 Fe 0 .2 Mn 0 .2 and in particular TiV 1 .6 Fe 0 .4, TiV 1 .5 Fe 0 .4 Mn 0 .1, and TiV 1 .6 Fe 0 .2 Cr 0 .1 Mn 0 .1.
  • the greater material described have remarkably low absorption pressures of less than 10 -6 mbar and are frequently within the order of 10 -7 -10 -8 mbar.
  • the getter materials are particularly inexpensive to prepare, for example using inexpensive ferrovanadium.
US06/751,972 1984-07-07 1985-07-05 Titanium-based alloy used as a gettering material Expired - Lifetime US4717551A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3425055A DE3425055C1 (de) 1984-07-07 1984-07-07 Getterstoff
DE3425055 1984-07-07

Publications (1)

Publication Number Publication Date
US4717551A true US4717551A (en) 1988-01-05

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Family Applications (1)

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US06/751,972 Expired - Lifetime US4717551A (en) 1984-07-07 1985-07-05 Titanium-based alloy used as a gettering material

Country Status (5)

Country Link
US (1) US4717551A (de)
DE (1) DE3425055C1 (de)
FR (1) FR2567154B1 (de)
GB (1) GB2161182B (de)
IT (1) IT1188172B (de)

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4973227A (en) * 1988-06-16 1990-11-27 HWT Gesellschaft fur Hydrid-und Wasserstofftechnik m.b.H. Method of producing a vacuum
US5489327A (en) * 1994-03-04 1996-02-06 Japan Pionics Co., Ltd. Process for purifying hydrogen gas
US5669961A (en) * 1993-07-12 1997-09-23 Lockheed Martin Idaho Technologies Company Method for the purification of noble gases, nitrogen and hydrogen
US5833738A (en) * 1996-03-01 1998-11-10 D.D.I. Ltd. Specialty gas purification system
US5985007A (en) * 1995-07-21 1999-11-16 D.D.I. Ltd. Noble gas purifier with single purifier vessel and recuperative heat exchanger
US20040040941A1 (en) * 2002-09-03 2004-03-04 Ecklund Steven P. Methods and apparatus for removing gases from enclosures
US20080199350A1 (en) * 2001-11-22 2008-08-21 Tetyukhin Vladislav Valentinov Metastable beta-titanium alloy
CN102810440A (zh) * 2012-08-02 2012-12-05 中国航天科工集团第二研究院二〇三所 一种制备氢原子频标的吸气片工艺方法
ITMI20122092A1 (it) * 2012-12-10 2014-06-11 Getters Spa Leghe getter non evaporabili riattivabili dopo l'esposizione a gas reattivi
US10583486B2 (en) 2017-01-04 2020-03-10 Honeywell International Inc. Hot isostatic pressing apparatus and hot isostatic pressing methods for reducing surface-area chemical degradation on an article of manufacture

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3436754C1 (de) * 1984-10-06 1985-08-14 Daimler-Benz Ag, 7000 Stuttgart Mittel zur Aufrechterhaltung des Vakuums im Vakuummantel von thermischen Isolierbehaeltern
RU2073737C1 (ru) * 1994-12-29 1997-02-20 Товарищество с ограниченной ответственностью "Техновак +" Нераспыляемый ленточный газопоглотитель и способ его получения
US5814241A (en) * 1994-12-29 1998-09-29 Tovarischetstvo S Organichennoi Otvetstvennostju "Tekhnovakt" Non-vaporizing getter and method of obtaining the same

Citations (15)

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Publication number Priority date Publication date Assignee Title
US30083A (en) * 1860-09-18 Apparatus for cleaning
US3005698A (en) * 1959-04-09 1961-10-24 Titanium Metals Corp Producing brittle titanium metal
US3627521A (en) * 1969-02-28 1971-12-14 Crucible Inc Method of forming a powdered-metal compact employing a beta-titanium alloy as a getter for gaseous impurities
US3992685A (en) * 1972-09-05 1976-11-16 Trw Systems & Energy Chemical laser pump
US4069303A (en) * 1976-02-20 1978-01-17 Matsushita Electric Industrial Company Alloy useful as hydrogen storage material
US4111689A (en) * 1976-02-09 1978-09-05 Franklin Baumgartner Method of storing hydrogen
US4154364A (en) * 1975-12-30 1979-05-15 Shin-Etsu Chemical Co., Ltd. Thermally insulating containers for liquefied gases
US4278466A (en) * 1978-11-14 1981-07-14 Battelle Memorial Institute Titanium alloy composition and method for the storage of hydrogen
US4358316A (en) * 1980-12-29 1982-11-09 University Patents, Inc. Alloys for hydrogen storage
US4360445A (en) * 1981-06-16 1982-11-23 The United States Of America As Represented By The United States Department Of Energy Oxygen stabilized zirconium-vanadium-iron alloy
US4397834A (en) * 1980-10-14 1983-08-09 Mendelsohn Marshall H Method of gettering hydrogen under conditions of low pressure
GB2117002A (en) * 1982-03-20 1983-10-05 Daimler Benz Ag Hydrogen storage material
GB2123805A (en) * 1982-06-28 1984-02-08 Getters Spa Separating hydrogen isotopes
US4440736A (en) * 1982-09-20 1984-04-03 Allied Corporation Titanium-based body-centered cubic phase alloy compositions and room temperature hydride-forming reactions of same
US4446101A (en) * 1981-10-03 1984-05-01 Daimler-Benz Aktiengesellschaft Storage material for hydrogen

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NL272643A (de) * 1961-04-24
GB964566A (en) * 1961-08-17 1964-07-22 Volvo Ab Improvements in or relating to gas turbine power plants
GB1175683A (en) * 1966-05-10 1969-12-23 Imp Metal Ind Kynoch Ltd Improvements in or relating to Titanium-Base Alloys
DE2010871A1 (de) * 1970-03-07 1971-10-07 Kernforschung Gmbh Ges Fuer Gegen Kernbrennstoff und Reaktorkuhl mittel korrosionsbeständige Brennstoff hülle fur Kernreaktoren
CH527412A (de) * 1970-07-17 1972-08-31 Straumann Inst Ag Spannband für die Spannbandaufhängung eines drehbaren Messwerks
NL7513159A (nl) * 1975-11-11 1977-05-13 Philips Nv Titaan en ijzer bevattend materiaal voor het opslaan van waterstof.

Patent Citations (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US30083A (en) * 1860-09-18 Apparatus for cleaning
US3005698A (en) * 1959-04-09 1961-10-24 Titanium Metals Corp Producing brittle titanium metal
US3627521A (en) * 1969-02-28 1971-12-14 Crucible Inc Method of forming a powdered-metal compact employing a beta-titanium alloy as a getter for gaseous impurities
US3992685A (en) * 1972-09-05 1976-11-16 Trw Systems & Energy Chemical laser pump
US4154364A (en) * 1975-12-30 1979-05-15 Shin-Etsu Chemical Co., Ltd. Thermally insulating containers for liquefied gases
US4111689A (en) * 1976-02-09 1978-09-05 Franklin Baumgartner Method of storing hydrogen
US4069303A (en) * 1976-02-20 1978-01-17 Matsushita Electric Industrial Company Alloy useful as hydrogen storage material
US4278466A (en) * 1978-11-14 1981-07-14 Battelle Memorial Institute Titanium alloy composition and method for the storage of hydrogen
US4397834A (en) * 1980-10-14 1983-08-09 Mendelsohn Marshall H Method of gettering hydrogen under conditions of low pressure
US4358316A (en) * 1980-12-29 1982-11-09 University Patents, Inc. Alloys for hydrogen storage
US4360445A (en) * 1981-06-16 1982-11-23 The United States Of America As Represented By The United States Department Of Energy Oxygen stabilized zirconium-vanadium-iron alloy
US4446101A (en) * 1981-10-03 1984-05-01 Daimler-Benz Aktiengesellschaft Storage material for hydrogen
GB2117002A (en) * 1982-03-20 1983-10-05 Daimler Benz Ag Hydrogen storage material
GB2123805A (en) * 1982-06-28 1984-02-08 Getters Spa Separating hydrogen isotopes
US4440736A (en) * 1982-09-20 1984-04-03 Allied Corporation Titanium-based body-centered cubic phase alloy compositions and room temperature hydride-forming reactions of same

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
Boffito et al., "A Nonevaporable Low Temperature Activatable Getter Material", J. Vac. Sci. Technol., 18(3), Apr. 1981, pp. 1117-1120.
Boffito et al., A Nonevaporable Low Temperature Activatable Getter Material , J. Vac. Sci. Technol., 18(3), Apr. 1981, pp. 1117 1120. *
Mendelsohn et al., "Intermetallic Alloys as Bulk Getters" Proc. Intl. Symp. on Properties & Applications of Metal Hydrides, Colorado Springs, Co., Apr. 7-11, 1980.
Mendelsohn et al., Intermetallic Alloys as Bulk Getters Proc. Intl. Symp. on Properties & Applications of Metal Hydrides, Colorado Springs, Co., Apr. 7 11, 1980. *

Cited By (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4973227A (en) * 1988-06-16 1990-11-27 HWT Gesellschaft fur Hydrid-und Wasserstofftechnik m.b.H. Method of producing a vacuum
US5669961A (en) * 1993-07-12 1997-09-23 Lockheed Martin Idaho Technologies Company Method for the purification of noble gases, nitrogen and hydrogen
US5489327A (en) * 1994-03-04 1996-02-06 Japan Pionics Co., Ltd. Process for purifying hydrogen gas
US5985007A (en) * 1995-07-21 1999-11-16 D.D.I. Ltd. Noble gas purifier with single purifier vessel and recuperative heat exchanger
US5833738A (en) * 1996-03-01 1998-11-10 D.D.I. Ltd. Specialty gas purification system
US20080199350A1 (en) * 2001-11-22 2008-08-21 Tetyukhin Vladislav Valentinov Metastable beta-titanium alloy
US20040040941A1 (en) * 2002-09-03 2004-03-04 Ecklund Steven P. Methods and apparatus for removing gases from enclosures
US6931711B2 (en) 2002-09-03 2005-08-23 Honeywell International Inc. Methods and apparatus for removing gases from enclosures
CN102810440A (zh) * 2012-08-02 2012-12-05 中国航天科工集团第二研究院二〇三所 一种制备氢原子频标的吸气片工艺方法
CN102810440B (zh) * 2012-08-02 2014-12-03 中国航天科工集团第二研究院二〇三所 一种制备氢原子频标的吸气片工艺方法
ITMI20122092A1 (it) * 2012-12-10 2014-06-11 Getters Spa Leghe getter non evaporabili riattivabili dopo l'esposizione a gas reattivi
WO2014091355A1 (en) * 2012-12-10 2014-06-19 Saes Getters S.P.A. Non-evaporable getter alloys reactivable after exposure to reactive gases
KR20150065953A (ko) * 2012-12-10 2015-06-15 사에스 게터스 에스.페.아. 반응성 가스에 노출 후 재활성화될 수 있는 비-증발성 게터 합금
US9064668B2 (en) 2012-12-10 2015-06-23 Saes Getters S.P.A. Non-evaporable getter alloys reactivable after exposure to reactive gases
CN104871284A (zh) * 2012-12-10 2015-08-26 工程吸气公司 暴露于反应性气体之后可再活化的非蒸散型吸气剂合金
CN104871284B (zh) * 2012-12-10 2016-10-12 工程吸气公司 暴露于反应性气体之后可再活化的非蒸散型吸气剂合金
US10583486B2 (en) 2017-01-04 2020-03-10 Honeywell International Inc. Hot isostatic pressing apparatus and hot isostatic pressing methods for reducing surface-area chemical degradation on an article of manufacture

Also Published As

Publication number Publication date
IT1188172B (it) 1988-01-07
GB2161182A (en) 1986-01-08
FR2567154A1 (fr) 1986-01-10
IT8521297A0 (it) 1985-06-26
GB2161182B (en) 1988-09-01
FR2567154B1 (fr) 1992-12-31
DE3425055C1 (de) 1985-07-25
GB8516713D0 (en) 1985-08-07

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